CN102246945A - Resource and harmless processing method for biggest solid waste distiller's grain of traditional white spirit - Google Patents

Resource and harmless processing method for biggest solid waste distiller's grain of traditional white spirit Download PDF

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CN102246945A
CN102246945A CN2011101197776A CN201110119777A CN102246945A CN 102246945 A CN102246945 A CN 102246945A CN 2011101197776 A CN2011101197776 A CN 2011101197776A CN 201110119777 A CN201110119777 A CN 201110119777A CN 102246945 A CN102246945 A CN 102246945A
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fermentation
solid
steamer
poor
temperature
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CN102246945B (en
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季良威
李平
王领
钟秀训
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Sichuan Yinfan Biotechnology Co Ltd
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Sichuan Yinfan Biotechnology Co Ltd
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Abstract

The invention discloses a resource and harmless processing method for biggest solid waste distiller's grain of traditional white spirit. The method comprises the following steps: adding diastatic enzyme, acid protease, thermostable active dry yeast, moderate-temperature yeast and cellulase into the distiller's grain of white spirit, and putting the mixture in a pit for solid state fermentation; adding rhizopus, red yeast, high-temperature yeast, distiller's grain wine and concentrated hexanoic acid fermentation liquid into the pit for solid-liquid combined fermentation; extracting and distilling the fermented grains to obtain natural essence for thick-flavor white spirit, natural essence for table vinegar and substance prepared into protein feed at the same time. The method disclosed by the invention has low cost, short production period, can process 35,000 tons of distiller's grain annually for the production scale of 8,000 t/a, reduces the pollutants CODcr, BOD5, SS and ammonia nitrogen discharged to environment, and plays a tremendous effect in the regional environmental protection. Meanwhile, the essence products prepared from the distiller's grain effectively improve the quality of white spirit and table vinegar, and sufficiently reflect the recycling value of the resource and harmless processing of solid waste of white spirit.

Description

The maximum solid waste of traditional liquor is lost poor resource and method for innocent treatment
Technical field
The present invention relates to a kind of brewed spirit recycling of solid wastes and harmless processing method, belong to the environmental protection field.
Background technology
We know that the production of conventional solid-state liquor is that a multistep is rapid, the process that the production cycle is long, and 1 ton of 60 former wine of degree of every output, there then have the 3-4 ton to lose to be poor.Owing to lose the strong suction-operated of precipitation, cellulose, hemicellulose in poor, water and many organic matters all be wrapped in lose poor in.Generally lose poor the stacking after 2 days, because air and action of microorganisms, a large amount of organic wastewaters ooze out, and its average CODcr is up to 5.65*10 5Mg/L.Generally speaking, middle-size and small-size wine industry will be lost to be pickled with grains or in wine and be sold when running up to some.Cause local water environment pollution inevitably losing in the poor holdup time.Large-scale wine enterprise all adopts and drops into environmental protection facility voluntarily and handle.
Owing in the spirit distiller grain, except that the flavor component that contains liquor, also be rich in starch, crude protein, crude fat, carbohydrate, cellulose, calcium, phosphorus, iron, amino acid, except that starch, high energy composition homogeneous phases such as crude protein, crude fat are similar to corn in dried being pickled with grains or in wine.Therefore, the domestic approach that utilizes to spirit distiller grain has following several mode:
1, produce high protein feed, the technology of taking is: lose poor → solid-liquid initial gross separation → drying (140 ~ 160 ℃) pulverizing → sale.In implementing dry run, generally use the hot blast drum drying machine, fluidized bed dryer or air-flowing type drying.This kind method also will be to the further biochemical treatment of isolated organic wastewater.In drying, many flavor components and organic matter are discharged, and cause air pollution.
2, produce biogas, adopting process is: lose poor → Separation of Solid and Liquid → poor liquid through anaerobism → anaerobic fermentation → biogas.Produce the mode of biogas and only utilized poor liquid, but residual poor slag still need handle, the cripple amount behind the biochemical biogas is big, and the CODcr after the processing also needs the secondary biochemical treatment could qualified discharge generally about 10000mgL.This method is disposable to have high input, the operating cost height.
3, it is fertile to make farming, and adopting process is: it is personal to lose poor → Separation of Solid and Liquid → mix pond sludge → peasant.Though can change barren soil clay structure, increase organic matter, improve land fertility, make agricultural produce, this method still drains into atmosphere with many organic matters.If be used for Edible Fungi, cultivate the environmental pollution that body also can cause the secondary solid discarded object, income is very little economically.
4, be used for aquaculture, will lose the poor heap fermentation after the acidity of suitably adjusting, allow can excite organic matter to discharge after, culture fly maggot, earthworm etc.Also have to utilize and lose the poor forage protein that extracts, produce processing methods such as glycerine.
More than these methods lose poor environmental pollution and have certain effect solving the wine brewing solid waste, but income is very little economically.And in the China that has the very huge liquor consumer group, accessory substance and discarded object by liquor self fermentation, produce fermented soy baste (natural essence), all will produce enormous function to social benefit and economic benefit undoubtedly, especially the maximum solid waste of liquor is lost poor method for innocent treatment and be there is no relevant report at present at home and abroad.
Summary of the invention
The object of the present invention is to provide the maximum solid waste of a kind of liquor to lose poor resource and method for innocent treatment, residual shallow lake during its utilization is lost and is pickled with grains or in wine, residual sugar, earlier through carbohydrase, cellulase, acid protease, high temperature resistant active dry yeast and daqu of middle temperature effect, carry out solid state fermentation, again by adding based on head mold, red colouring agent for food, also used as a Chinese medicine, high-temperature daqu is the compound esterification enzyme and the concentrated caproic acid fermentation liquid of assisting, carry out the solid-liquid combination fermentation, obtain containing abundant ester respectively, the aromatic Chinese spirit of local flavors such as aldehyde ketone with and vinegar with brewageing baste, residue can be made into protein feed, thereby reaches the purpose that the maximum solid waste of liquor is lost poor harmless treatment.
The objective of the invention is that following technical scheme realizes by implementing.
The maximum solid waste of a kind of liquor is lost poor resource and method for innocent treatment, it is characterized in that it is is raw material to lose poor, obtains aromatic Chinese spirit simultaneously and is used to make protein feed with natural essence, vinegar with natural essence and remaining residue by solid state fermentation, solid-liquid combination fermentation, extractive distillation:
A, solid state fermentation stage
To lose poor evenly placing in the white spirit distiller, with 100 ~ 110 ℃ of saturated vapor dry blowing 15 ~ 30min, following rice steamer, airing is waited to lose the temperature that is pickled with grains or in wine and is reduced to 59 ~ 61 ℃, is spilled into the carbohydrase behind the water activation, mixes thoroughly; Continue airing and be cooled to 45 ~ 50 ℃, be spilled into the cellulase behind the water activation again, and add acid protease, mix thoroughly; Further airing is cooled to 28 ~ 30 ℃, be spilled into the high temperature resistant active brewer's dried yeast activating solution behind the water activation, and account for the daqu of middle temperature of losing poor weight 2%, mix evenly after, go into to store in 28 ~ 33 ℃ temperature bottom fermentation 12 ~ 16 days, unstrained spirits must be pickled with grains or in wine.
Described to lose poor residual shallow lake content be 9.2%(W/W).
Carbohydrase behind the described water activation is: by weight, will account for lose poor in the carbohydrase of starch 200 ~ 240u/g to be dissolved in 15 ~ 20 times, temperature be to activate 30 ~ 60min promptly in 30 ~ 35 ℃ the water.
Cellulase behind the described water activation is: by weight, will account for and lose poor weight 0.12% ~ 0.15% cellulase to be dissolved in 15 ~ 20 times, temperature be to activate 30 ~ 60min promptly in 40 ~ 45 ℃ the water.
High temperature resistant active brewer's dried yeast activating solution behind the described water activation is: by weight, will accounting for the high temperature resistant active brewer's dried yeast of losing poor weight 0.15 ~ 0.2%, to be dissolved in 20 ~ 25 times, temperature be that 38 ~ 40 ℃, concentration are 2%(w/w) sucrose solution in activate 30 ~ 60min promptly.
The addition of described acid protease is that 14 ~ 20u/g loses poor raw material.
Described carbohydrase, cellulase, acid protease, high temperature resistant active brewer's dried yeast are the commercially available prod, wherein the enzymatic activity of carbohydrase is 40000 ~ 50000u/g, and the product enzyme enzyme of cellulase (CMC) alive is that the enzymatic activity of 800 ~ 908u/g, acid protease is 50000 ~ 60000u/g.
The all right green wooden enzyme of described cellulase ( Trichoderma viride) be starting strain, obtain through solid state fermentation.
The wooden enzyme of described green ( Trichoderma viride) deriving from DSMZ of Institute of Micro-biology of the Chinese Academy of Sciences, its deposit number is 3.1044.
The process conditions of described solid state fermentation are: siccative: water=1: 1, and wherein, the composition of siccative and proportioning are: straw: wheat bran=6 ~ 7: 4 ~ 3, charge 7 ~ 8%, inoculum concentration 3 ~ 5%, 36 ~ 40 ℃ of cultivation temperature, fermentation period 72 ~ 80h; All ratios are weight ratio.
The granularity of the daqu of middle temperature after the described pulverizing is 200 ~ 300 orders.
B, solid-liquid combination fermentation stage
In the poor unstrained spirits behind solid state fermentation, add 6 ~ 8% compound esterification enzyme and 6 ~ 8% high-temperature daqu by weight, after mixing thoroughly, under 30 ~ 45 ℃ of temperature, pile up 18 ~ 24h, the arrack of losing that adds 9 ~ 10% concentrated caproic acid fermentation liquid and 10 ~ 15% again, last pit entry fermentation got the wine unstrained spirits in 6 ~ 8 days, and fermentation temperature is 36 ~ 40 ℃.
Described compound esterification enzyme by head mold and Monascus ruber by 7 ~ 6: 3 ~ 4 weight ratio mixes.
The caproic acid content of described concentrated caproic acid fermentation liquid is 28g/L.
The described arrack of losing is 50% ~ 60% vol.。
C, extractive distillation
The wine unstrained spirits that obtains after solid-liquid combination fermentation is packed in the white spirit distiller, adds hot reflux 30 ~ 40min under 0.015 ~ 0.02Mpa pressure, collects distillate, raffinate and solid residue respectively, to realize resource and harmless treatment;
Wherein,
A, the distillate head section of heating up in a steamer, the centre section of heating up in a steamer, rear are collected respectively, and respectively the section of heating up in a steamer is respectively charged in the steam distillation device, distillates 38 ~ 45%(V/V) under 0.1 ~ 0.15Mpa steam, lasts 1.5 ~ 2h; Remaining part open vavuum pump-0.05 ~-0.06Mpa pressure carries out decompression distillation, lasts 0.5 ~ 0.8h; Last remaining raffinate directly enters sewage disposal system, enters circulation after treatment again; Wherein, the distillate head section of heating up in a steamer: the centre section of heating up in a steamer: the weight ratio of rear=11% ~ 15%:65% ~ 69%:16% ~ 20% makes up composite, and the storage tank of packing into is deposited naturally and obtained aromatic Chinese spirit natural essence product after 5 ~ 8 days.
The described head section of heating up in a steamer, the centre section of heating up in a steamer, rear are the divisions that the wine degree by distillate carries out, and wherein a section of heating up in a steamer is that 60.8 ~ 75.4% vol, the centre section of heating up in a steamer are that 21.5 ~ 60.8% vol, rear are 4.1 ~ 21.5% vol.
The described CODcr that enters the sewage disposal system raffinate is 2000 ~ 3000mg/L.
The described CODcr that enters the circulation raffinate after treatment is 60 ~ 90 mg/L.
B, raffinate are under 50 ~ 80 ℃ of temperature, the active carbon that adds raffinate weight 0.1% ~ 0.15%, leave standstill 6 ~ 10h, after coarse filtration and smart filter obtain little brown, transparence filtrate, filtrate and the head section of heating up in a steamer, the centre section of heating up in a steamer, the rear collected are carried out the composite vinegar natural essence product that promptly obtains by the weight ratio of 80% ~ 85%:3% ~ 9%:5% ~ 7%:5% ~ 9% respectively.
C, solid residue are directly sold and are used to make protein feed.
Described aromatic Chinese spirit with natural essence product and vinegar with the component content testing result of natural essence see Table 1 respectively, table 2:
Table 1 unit: mg/100ml
Figure 550366DEST_PATH_IMAGE001
Figure 281562DEST_PATH_IMAGE002
Described white spirit distiller is split-type structural, comprise Zeng Gai, rice steamer bucket, end pot and rice steamer comb, wherein the rice steamer bucket comprises upper strata rice steamer bucket and lower floor's rice steamer bucket, upper strata rice steamer bucket and lower floor rice steamer bucket upper end all are welded with zigzag taper brine collecting ring to overcome wall effect, the junction of upper strata rice steamer bucket and lower floor's rice steamer bucket is provided with gasket seal, the bottom of upper strata rice steamer bucket and lower floor's rice steamer bucket is provided with rice steamer and combs, and described rice steamer comb is connected to form by the rice steamer comb body of two semicirculars in shape; Rice steamer covers the interior reflux that is provided with the taper coiled pipe cooler, and part alcohol in high concentration cooling back is extracted the poor unstrained spirits in upper strata; One cover external reflux device also is set, stretches into the rice steamer body and be divided into the cross backflow distributor that has aperture, the uncolled high wine vapour that refluxes in the part after the heat exchanger cooling, passes back in the rice steamer body by external reflux device, and the poor unstrained spirits of lower floor is extracted.The concrete operations step of this distiller and method see for details with patent application of the present invention in the utility model patent of declaring to State Intellectual Property Office on the same day---" white spirit distiller ".
Useful technique effect of the present invention shows:
1, utilizes and lose poor residual shallow lake, residual sugar in the traditional liquor production, and the aromatic Chinese spirit natural essence by solid-liquid combination fermentation preparation, both can be in traditional liquor, use as special blending liquor, the natural flavor composition that also can be used as white spirit uses, thereby avoided adding " floating fragrant " that synthon spices brings, strengthened the sense and the solid-state sense naturally of liquor, promoted the quality of white spirit.
2, by the wine unstrained spirits being taked stage extraction distillation, thereby reduce the wine damage, improved the recovery rate of flavor component.
3, look forward to the production blending liquor with existing wine and compare, the production cycle can shorten 30 days at least.
4, cost is low, and the four seasons all can produce, and saves labor hour more than 60%.
5,, can reach a year processing and lose poor 35000t, and reduce amount of pollutant CODcr 178.8t/a, the BOD that discharging enters environment as forming production scale 8000t/a product 5809.2t/a, SS 359.8t/a, ammonia nitrogen 1.426t/a, thereby huge effect has been played in regional environmental protection.
6, through solid state fermentation after the stage, lose poor remaining content of starch and reduce to 2.1%, remaining starch utilization ratio reaches 77%, every 100Kg loses the poor average 60%(vol of producing) about wine 5.46Kg, lose at aroma daqu liquor therefore that to use cellulase, carbohydrase, high temperature resistant active brewer's dried yeast and the acid protease generation alcohol effect of fermenting once more in poor remarkable.
7, utilize and lose poor residual shallow lake, residual sugar in the traditional liquor production, and the vinegar natural essence by solid-liquid combination fermentation preparation, its security is good, can better improve the quality of vinegar.
8, solid residue has realized the recycle value of liquor solid-state castoff resource well as protein feed.
The specific embodiment
Embodiment 1 The solid state fermentation stage
To lose poor evenly placing in the white spirit distiller, with 100 ℃ of saturated vapor dry blowing 20min, following rice steamer, airing is waited to lose the temperature that is pickled with grains or in wine and is reduced to 60 ℃, is spilled into the carbohydrase behind the water activation, mixes thoroughly; Continue airing and be cooled to 50 ℃, be spilled into the cellulase behind the water activation again, and add acid protease, mix thoroughly; Further airing is cooled to 30 ℃, spills the high temperature resistant active brewer's dried yeast activating solution after the people accounts for water activation again, and accounts for the daqu of middle temperature of losing poor weight 2%, mix evenly after, go into to store in 28 ~ 30 ℃ temperature bottom fermentation 16 days, unstrained spirits must be pickled with grains or in wine.
Described to lose poor residual shallow lake content be 9.2%(W/W).
Carbohydrase behind the described water activation is: by weight, with account for lose poor in the carbohydrase of starch 200u/g to be dissolved in 15 times, temperature be that activation 40min is promptly in 30 ℃ the water.
Cellulase behind the described water activation is: by weight, to be dissolved in 20 times, temperature be that activation 30min is promptly in 40 ℃ the water with accounting for the cellulase of losing poor weight 0.15%.
High temperature resistant active brewer's dried yeast activating solution behind the described water activation is: by weight, to be dissolved in 20 times, temperature be that 40 ℃, concentration are 2%(w/w with accounting for the high temperature resistant active brewer's dried yeast of losing poor weight 0.2%) sucrose solution in activation 60min promptly.
The addition of described acid protease is that 20u/g loses poor raw material.
Described carbohydrase, cellulase, acid protease, high temperature resistant active brewer's dried yeast are the commercially available prod, wherein the enzymatic activity of carbohydrase is 40000 ~ 50000u/g, and the product enzyme enzyme of cellulase (CMC) alive is that the enzymatic activity of 800 ~ 908u/g, acid protease is 50000 ~ 60000u/g.
The granularity of the daqu of middle temperature after the described pulverizing is 200 ~ 300 orders.
The 2 solid state fermentation stages of embodiment
To lose poor evenly placing in the white spirit distiller, with 110 ℃ of saturated vapor dry blowing 15min, following rice steamer, airing is waited to lose the temperature that is pickled with grains or in wine and is reduced to 59 ℃, is spilled into the carbohydrase behind the water activation, mixes thoroughly; Continue airing and be cooled to 45 ℃, be spilled into the cellulase behind the water activation again, and add acid protease, mix thoroughly; Further airing is cooled to 28 ℃, spills the high temperature resistant active brewer's dried yeast activating solution after the people accounts for water activation again, and accounts for the daqu of middle temperature of losing poor weight 2%, mix evenly after, go into to store in 30 ~ 33 ℃ temperature bottom fermentation 12 days, unstrained spirits must be pickled with grains or in wine.
Described to lose poor residual shallow lake content be 9.2%(W/W).
Carbohydrase behind the described water activation is: by weight, with account for lose poor in the carbohydrase of starch 240u/g to be dissolved in 20 times, temperature be that activation 30min is promptly in 32 ℃ the water.
Cellulase behind the described water activation is: by weight, to be dissolved in 15 times, temperature be that activation 50min is promptly in 45 ℃ the water with accounting for the cellulase of losing poor weight 0.12%.
High temperature resistant active brewer's dried yeast activating solution behind the described water activation is: by weight, to be dissolved in 25 times, temperature be that 38 ℃, concentration are 2%(w/w with accounting for the high temperature resistant active brewer's dried yeast of losing poor weight 0.15%) sucrose solution in activation 30min promptly.
The addition of described acid protease is that 14u/g loses poor raw material.
Described carbohydrase, acid protease, high temperature resistant active brewer's dried yeast are the commercially available prod, and wherein the enzymatic activity of carbohydrase is 40000 ~ 50000u/g, and the enzymatic activity of acid protease is 50000 ~ 60000u/g.
Described cellulase be with the wooden enzyme of green ( Trichoderma viride) be starting strain, obtain through solid state fermentation, it produces enzyme enzyme (CMC) alive is 800 ~ 908u/g.
The wooden enzyme of described green ( Trichoderma viride) deriving from DSMZ of Institute of Micro-biology of the Chinese Academy of Sciences, its deposit number is 3.1044.
The process conditions of described solid state fermentation are: siccative: water=1: 1, and wherein, the composition of siccative and proportioning are: straw: wheat bran=6 ~ 7: 4 ~ 3, charge 7 ~ 8%, inoculum concentration 3 ~ 5%, 36 ~ 40 ℃ of cultivation temperature, fermentation period 72 ~ 80h; All ratios are weight ratio.
The granularity of the daqu of middle temperature after the described pulverizing is 200 ~ 300 orders.
Embodiment 3 solid-liquid combination fermentation stages
In the poor unstrained spirits that embodiment 1 makes, add 6% compound esterification enzyme and 8% high-temperature daqu by weight, after mixing thoroughly, under 35 ℃ of temperature, pile up 24h, the arrack of losing that adds 10% concentrated caproic acid fermentation liquid and 15% again, last pit entry fermentation 8 days the wine unstrained spirits, fermentation temperature is 36 ~ 40 ℃.
Described compound esterification enzyme is mixed by head mold and the Monascus ruber weight ratio by 7: 4.
The caproic acid content of described concentrated caproic acid fermentation liquid is 28g/L, takes from Sichuan Yinfan Biotechnology Co., Ltd.'s fermentation plant.
The described arrack of losing is 57% vol, takes from Sichuan Yinfan Biotechnology Co., Ltd. liquor experiment base.
Embodiment 4 solid-liquid combination fermentation stages
In the poor unstrained spirits that embodiment 2 makes, add 7% compound esterification enzyme and 6% high-temperature daqu by weight, after mixing thoroughly, under 45 ℃ of temperature, pile up 18h, the arrack of losing that adds 9% concentrated caproic acid fermentation liquid and 10% again, last pit entry fermentation 6 days the wine unstrained spirits, fermentation temperature is 36 ~ 40 ℃.
Described compound esterification enzyme is mixed by head mold and the Monascus ruber weight ratio by 6: 3.
The caproic acid content of described concentrated caproic acid fermentation liquid is 28g/L, takes from Sichuan Yinfan Biotechnology Co., Ltd.'s fermentation plant.
The described arrack of losing is 60% vol, takes from Sichuan Yinfan Biotechnology Co., Ltd. liquor experiment base.
Embodiment 5 extractive distillations
The wine unstrained spirits that embodiment 3 is obtained is packed in the white spirit distiller, adds hot reflux 30 ~ 40min under 0.015 ~ 0.02Mpa pressure, collects distillate, raffinate and solid residue respectively, to realize resource and harmless treatment; Wherein, the distillate head section of heating up in a steamer, the centre section of heating up in a steamer, rear are collected respectively, the described head section of heating up in a steamer, the centre section of heating up in a steamer, rear are the divisions that the wine degree by distillate carries out, and a section of heating up in a steamer is that 60.8 ~ 75.4% vol, the centre section of heating up in a steamer are that 21.5 ~ 60.8% vol, rear are 4.1 ~ 21.5% vol; Solid residue is directly sold and is used to make protein feed.
Embodiment 6 extractive distillations
The wine unstrained spirits that embodiment 4 is obtained is packed in the white spirit distiller, adds hot reflux 40min under 0.015Mpa pressure, collects distillate, raffinate and solid residue respectively, to realize resource and harmless treatment;
Wherein, the distillate head section of heating up in a steamer, the centre section of heating up in a steamer, rear are collected respectively, the described head section of heating up in a steamer, the centre section of heating up in a steamer, rear are the divisions that the wine degree by distillate carries out, and a section of heating up in a steamer is that 60.8 ~ 75.4% vol, the centre section of heating up in a steamer are that 21.5 ~ 60.8% vol, rear are 4.1 ~ 21.5% vol; Solid residue is directly sold and is used to make protein feed.
Embodiment 7 concentrates, combination, composite
Each section distillate that embodiment 5 is collected is respectively charged in the steam distillation device, distillates 40%(V/V under 0.1Mpa steam), last 2h; Remaining part open vavuum pump-0.05 ~-0.06Mpa pressure carries out decompression distillation, lasts 0.8h; Last remaining remaining liquid directly enters sewage disposal system, enter circulation after treatment again, the head section of heating up in a steamer after concentrating, the centre section of heating up in a steamer, rear then make up composite according to 12%, 68%, 20% weight ratio respectively, after the storage tank of packing into is deposited 5 ~ 8 days naturally, promptly obtain aromatic Chinese spirit natural essence product.
The described CODcr that enters the sewage disposal system raffinate is 2000 ~ 3000mg/L.
The described CODcr that enters the circulation raffinate after treatment is 60 ~ 90 mg/L.
Embodiment 8 decolourings, removal of impurities, combination, composite
The raffinate that embodiment 5 is collected is under 70 ℃ of temperature, the active carbon that adds raffinate weight 0.1%, leave standstill 8h, after coarse filtration and smart filter obtain little brown, transparence filtrate, again filtrate and the head section of heating up in a steamer, the centre section of heating up in a steamer, rear are undertaken obtaining vinegar natural essence product after composite by the weight ratio of 85%:5%:5%:5% respectively.

Claims (9)

1. the maximum solid waste of liquor is lost poor resource and method for innocent treatment, it is characterized in that it is is raw material to lose poor, by solid state fermentation, solid-liquid combination fermentation, extractive distillation obtain simultaneously aromatic Chinese spirit with natural essence, vinegar with natural essence and be used to make the material of protein feed:
The solid state fermentation stage
To lose poor evenly placing in the white spirit distiller, with 100 ~ 110 ℃ of saturated vapor dry blowing 15 ~ 30min, following rice steamer, airing is waited to lose the temperature that is pickled with grains or in wine and is reduced to 59 ~ 61 ℃, is spilled into the carbohydrase behind the water activation, mixes thoroughly; Continue airing and be cooled to 45 ~ 50 ℃, be spilled into the cellulase behind the water activation again, and add acid protease, mix thoroughly; Further airing is cooled to 28 ~ 30 ℃, spills the high temperature resistant active brewer's dried yeast activating solution after the people accounts for water activation again, and accounts for the daqu of middle temperature of losing poor weight 2%, mix evenly after, go into to store in 28 ~ 33 ℃ temperature bottom fermentation 12 ~ 16 days, unstrained spirits must be pickled with grains or in wine;
It is described that to lose poor residual shallow lake content be 9.2% by weight percentage;
Carbohydrase behind the described water activation is: by weight, will account for lose poor in the carbohydrase of starch 200 ~ 240u/g to be dissolved in 15 ~ 20 times, temperature be to activate 30 ~ 60min promptly in 30 ~ 35 ℃ the water;
Cellulase behind the described water activation is: by weight, will accounting for the cellulase of losing poor weight 0.12% ~ 0.15%, to be dissolved in 15 ~ 20 times, temperature be to activate 30 ~ 60min promptly in 40 ~ 45 ℃ the water;
High temperature resistant active brewer's dried yeast activating solution behind the described water activation is: by weight, will accounting for the high temperature resistant active brewer's dried yeast of losing poor weight 0.15 ~ 0.2%, to be dissolved in 20 ~ 25 times, temperature be that 38 ~ 40 ℃, concentration are 2%(w/w) sucrose solution in activate 30 ~ 60min promptly;
The addition of described acid protease is that 14 ~ 20u/g loses poor raw material;
B, solid-liquid combination fermentation stage
In the poor unstrained spirits behind solid state fermentation, add 6 ~ 8% compound esterification enzyme and 6 ~ 8% high-temperature daqu by weight, after mixing thoroughly, under 30 ~ 45 ℃ of temperature, pile up 18 ~ 24h, the arrack of losing that adds 9 ~ 10% concentrated caproic acid fermentation liquid and 10 ~ 15% again, last pit entry fermentation got the wine unstrained spirits in 6 ~ 8 days, and fermentation temperature is 36 ~ 40 ℃;
Described compound esterification enzyme by head mold and Monascus ruber by 7 ~ 6: 3 ~ 4 weight ratio mixes;
C, extractive distillation
The wine unstrained spirits that obtains after solid-liquid combination fermentation is packed in the white spirit distiller, adds hot reflux 30 ~ 40min under 0.015 ~ 0.02Mpa pressure, collects distillate, raffinate and solid residue respectively, to realize resource and harmless treatment;
Wherein,
A, the distillate head section of heating up in a steamer, the centre section of heating up in a steamer, rear are collected respectively, and respectively the section of heating up in a steamer is respectively charged in the steam distillation device, distillates 38 ~ 45%(V/V) under 0.1 ~ 0.15Mpa steam, lasts 1.5 ~ 2h; Remaining part open vavuum pump-0.05 ~-0.06Mpa pressure carries out decompression distillation, lasts 0.5 ~ 0.8h; Last remaining raffinate directly enters sewage disposal system, enters circulation after treatment again; Wherein, the distillate head section of heating up in a steamer: the centre section of heating up in a steamer: the weight ratio of rear=11% ~ 15%:65% ~ 69%:16% ~ 20% makes up composite, and the storage tank of packing into is deposited naturally and obtained aromatic Chinese spirit natural essence product after 5 ~ 8 days;
The described head section of heating up in a steamer, the centre section of heating up in a steamer, rear are the divisions that the wine degree by distillate carries out, and wherein a section of heating up in a steamer is that 60.8 ~ 75.4% vol, the centre section of heating up in a steamer are that 21.5 ~ 60.8% vol, rear are 4.1 ~ 21.5% vol;
B, raffinate are under 50 ~ 80 ℃ of temperature, the active carbon that adds raffinate weight 0.1% ~ 0.15%, leave standstill 6 ~ 10h, after coarse filtration and smart filter obtain little brown, transparence filtrate, filtrate and the head section of heating up in a steamer, the centre section of heating up in a steamer, the rear collected are carried out the composite vinegar natural essence product that promptly obtains by the weight ratio of 80% ~ 85%:3% ~ 9%:5% ~ 7%:5% ~ 9% respectively;
C, solid residue are directly sold and are used to make protein feed.
2. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 1, the enzymatic activity that it is characterized in that carbohydrase described in the steps A is 40000 ~ 50000u/g, and the product enzyme enzyme work of cellulase is that the enzymatic activity of 800 ~ 908u/g, acid protease is 50000 ~ 60000u/g.
3. the spirit distiller grain solid-liquid combination fermenting and producing liquor that utilizes according to claim 1 and 2 is with the method for natural essence, it is characterized in that described cellulase be with the wooden enzyme of green ( Trichoderma viride) be starting strain, obtain through solid state fermentation; The wooden enzyme of described green ( Trichoderma viride) deriving from DSMZ of Institute of Micro-biology of the Chinese Academy of Sciences, its deposit number is 3.1044.
4. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 3, the process conditions that it is characterized in that described solid state fermentation are: siccative: water=1: 1, wherein, the composition of siccative and proportioning are: straw: wheat bran=6 ~ 7: 4 ~ 3, charge 7 ~ 8%, inoculum concentration 3 ~ 5%, 36 ~ 40 ℃ of cultivation temperature, fermentation period 72 ~ 80h; All ratios are weight ratio.
5. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 1, the granularity of the daqu of middle temperature after it is characterized in that pulverizing described in the steps A is 200 ~ 300 orders.
6. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 1 is characterized in that the caproic acid content of concentrated caproic acid fermentation liquid described in the step B is 28g/L.
7. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 1, it is characterized in that losing described in the step B arrack is 55% ~ 60% vol.
8. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 1 is characterized in that the described CODcr that enters the sewage disposal system raffinate of step C is 2000 ~ 3000mg/L.
9. the method for utilizing spirit distiller grain solid-liquid combination fermenting and producing liquor with natural essence according to claim 1 is characterized in that the described CODcr that enters the circulation raffinate after treatment of step C is 60 ~ 90 mg/L.
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CN105728431A (en) * 2016-02-24 2016-07-06 齐芳 Cleaning technology for vinasse
CN106479802A (en) * 2016-10-08 2017-03-08 湖北枝江酒业股份有限公司 A kind of method rapidly and efficiently utilizing remaining starch in red wine dregs
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CN111269794A (en) * 2020-04-08 2020-06-12 劲牌有限公司 Atmospheric and vacuum distillation method for solid Xiaoqu liquor
CN111690707A (en) * 2020-07-27 2020-09-22 金徽酒股份有限公司 Method and production system for preparing humus and artificial aged pit mud by waste vinasse double-round fermentation

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CN103141666A (en) * 2013-03-28 2013-06-12 山东轻工业学院 Method for producing microbe feed probiotics by using white spirit vinasse
CN103141666B (en) * 2013-03-28 2014-04-16 山东轻工业学院 Method for producing microbe feed probiotics by using white spirit vinasse
CN105728431A (en) * 2016-02-24 2016-07-06 齐芳 Cleaning technology for vinasse
CN107177509A (en) * 2016-03-09 2017-09-19 浙江科技学院 A kind of method that utilization rice vinegar produced by fermenting waste residues produces Hongqu powder (red colouring agent)
CN106479802A (en) * 2016-10-08 2017-03-08 湖北枝江酒业股份有限公司 A kind of method rapidly and efficiently utilizing remaining starch in red wine dregs
CN108823051A (en) * 2018-07-03 2018-11-16 沈阳市岳君台黄酒酿造厂 A kind of technology of vinasse production white wine
CN108913427A (en) * 2018-07-17 2018-11-30 江南大学 It is a kind of to utilize jujube Spirit by-product production Jujube wine method
CN108841547A (en) * 2018-07-30 2018-11-20 中国科学院成都生物研究所 A kind of production method of natural vinosity fragrance
CN111269794A (en) * 2020-04-08 2020-06-12 劲牌有限公司 Atmospheric and vacuum distillation method for solid Xiaoqu liquor
CN111269794B (en) * 2020-04-08 2021-07-20 劲牌有限公司 Atmospheric and vacuum distillation method for solid Xiaoqu liquor
CN111690707A (en) * 2020-07-27 2020-09-22 金徽酒股份有限公司 Method and production system for preparing humus and artificial aged pit mud by waste vinasse double-round fermentation

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